EP1408141A1 - Methode pour la deposition galvanique des bronzes - Google Patents

Methode pour la deposition galvanique des bronzes Download PDF

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Publication number
EP1408141A1
EP1408141A1 EP02022718A EP02022718A EP1408141A1 EP 1408141 A1 EP1408141 A1 EP 1408141A1 EP 02022718 A EP02022718 A EP 02022718A EP 02022718 A EP02022718 A EP 02022718A EP 1408141 A1 EP1408141 A1 EP 1408141A1
Authority
EP
European Patent Office
Prior art keywords
electrolyte
tin
wetting agent
aromatic
added
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP02022718A
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German (de)
English (en)
Other versions
EP1408141B1 (fr
Inventor
Katrin Zschintzsch
Joachim Dr. Heyer
Marlies Dr. Kleinfeld
Stefan Schäfer
Ortrud Steinius
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
MacDermid Enthone Inc
Original Assignee
Enthone Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
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Application filed by Enthone Inc filed Critical Enthone Inc
Priority to ES02022718T priority Critical patent/ES2531163T3/es
Priority to EP02022718.7A priority patent/EP1408141B1/fr
Priority to KR1020057004846A priority patent/KR100684818B1/ko
Priority to PCT/EP2003/011229 priority patent/WO2004035875A2/fr
Priority to CN2003801012538A priority patent/CN1703540B/zh
Priority to JP2004544134A priority patent/JP4675626B2/ja
Priority to US10/531,142 priority patent/US20060137991A1/en
Publication of EP1408141A1 publication Critical patent/EP1408141A1/fr
Publication of EP1408141B1 publication Critical patent/EP1408141B1/fr
Application granted granted Critical
Anticipated expiration legal-status Critical
Revoked legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/56—Electroplating: Baths therefor from solutions of alloys
    • C25D3/58—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of copper
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/56—Electroplating: Baths therefor from solutions of alloys
    • C25D3/60—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of tin

Definitions

  • the present invention relates to a process for the electrodeposition of Bronzes, with which the substrate to be coated in an acidic electrolyte, at least tin and copper ions, an alkyl sulfonic acid and a wetting agent has, is metallized and the representation of such an electrolyte.
  • EP 1 111 097 A2 and US Pat. No. 6,176,996 B1 disclose acidic electrolytes and Process for the separation of high quality tin or tin alloys known at a higher deposition rate. These are to electrolytes containing at least two divalent metal salts of an organic Have sulfonic acid and from which solderable and corrosion resistant Coatings are deposited, which, for example, as a substitute for leaded, solderable coatings, in electrical engineering for the production of printed circuit boards etc. be used.
  • the invention is therefore based on the object of specifying a method for the deposition of bronzes, which allows a uniform deposition of at least tin and copper next to each other from an acidic electrolyte at much higher deposition rates over the methods known in the art.
  • adherent and non-porous bronze coatings with high copper contents and different decorative and mechanical properties should be deposited.
  • an acidic electrolyte for the deposition of such bronze coatings which have a high content of bivalent copper ions can be stable to oxidation-induced sludge formation over a extended period of time, and is economically and environmentally sound.
  • the object is inventively achieved by a method of the type mentioned, which is characterized in that the electrolyte is an aromatic, nonionic wetting agent is added.
  • the disadvantages known in the prior art are eliminated with the provision of a novel composition of the electrolyte and achieved in this way significantly better deposition results.
  • the implementation is simplified and made more economical. This too is mainly due to the advantageous composition of the electrolyte.
  • the process is carried out at room temperature or between 17 to 25 ° C and the substrate to be coated in a strongly acidic medium at a pH of ⁇ 1 metallized. In this temperature range, the electrolyte is particularly stable.
  • there are no costs for heating the electrolyte and also the metallized substrates need not be cooled down in a time and cost intensive manner.
  • deposition rates of 0.25 ⁇ m / min are achieved at a current density of 1 A / dm 2 , inter alia due to the pH value and the advantageous addition of at least one aromatic, nonionic wetting agent.
  • This can be increased by the increase of the metal content up to 7 A / dm 2 in the rack application and for pass-through systems even up to 120 A / dm 2 .
  • applicable current densities in a range of 0.1 to 120 A / dm 2 are achieved depending on the type of system.
  • Another advantage of the aromatic, nonionic wetting agent used is that by the advantageous wetting properties during the process of Electrolyte and / or the substrate in the electrolyte little to no movement must be in order to achieve the desired deposition results, so that to the use of additional devices for moving the electrolyte can be waived.
  • Particularly advantageous is the addition of 2 to 40 g / l of one or more aromatic, nonionic wetting agent, with particular preference ⁇ -naphtholethoxylate and / or Nonylphenolethoxylat be used.
  • the proposed method is thus advantageously and economically environmentally friendly to the cyanidic processes.
  • nonionic wetting agents possible, provided that the advantageous mode of action of the aromatic, support or even reinforce nonionic wetting agent.
  • polyethylene glycols and / or anionic surfactants as anionic and / or aliphatic, nonionic wetting agents to the electrolyte added.
  • the method according to the invention in particular by the special composition of the electrolyte characterized.
  • This contains essentially tin and copper ions, a Alkyl sulfonic acid and an aromatic, nonionic wetting agent.
  • stabilizers and / or complexing agents, anionic and / or nonionic, aliphatic wetting agents, antioxidants, brighteners as well be included in the electrolyte further metal salts.
  • the mainly for the inventive deposition of bronze in the Electrolytes introduced metals - tin and copper - can primarily as Salts of alkylsulfonic acids, preferably as methanesulfonates or as salts of Mineral acids, preferably present as sulfates.
  • tin salt becomes special preferably the Zinnmethansulfonat used in the electrolyte, which advantageously in an amount of 5 to 195 g / l of electrolyte, preferably 11 to 175 g / l electrolyte is added to the electrolyte. This corresponds to a mission from 2 to 75 g / l, preferably 4 to 67 g / l of divalent tin ions.
  • Copper salt is particularly preferably the Kupfermethansulfonat in the electrolyte used, which is advantageously in an amount of 8 to 280 g / l electrolyte, preferably 16 to 260 g / l electrolyte is added to the electrolyte. This corresponds to an input of 2 to 70 g / l, preferably 4 to 65 g / l of bivalent Copper ions.
  • the use of methanesulfonic acid turned out to be particularly advantageous out, as these on the one hand, an advantageous solubility of the metal salts conditional and on the other hand, due to their acidity, the setting of the for the Required process pH or facilitates.
  • methanesulfonic acid the advantageous property, essential to the stability of Bades contribute.
  • the electrolyte is at least added an additional metal and / or chloride.
  • the Metals lie the Metals in the form of their soluble salts.
  • the addition of zinc and / or bismuth affects the properties of the deposited coatings in the special size.
  • the zinc and / or bismuth introduced into the electrolyte Metals can be used primarily as salts of alkylsulfonic acids, preferably as Methanesulfonates or as salts of mineral acids, preferably as sulfates available.
  • the preferred zinc salt is the zinc sulfate in the electrolyte used, which is advantageously in an amount of 0 to 25 g / l electrolyte, preferably 15 to 20 g / l electrolyte is added to the electrolyte.
  • Bismuth salt is most preferably bismuth methanesulfonate in the electrolyte used, which is advantageously in an amount of 0 to 5 g / l electrolyte, preferably 0.05 to 0.2 g / l of electrolyte is added to the electrolyte.
  • electrolyte various additives, such as Stabilizers and / or complexing agents, antioxidants and brighteners, which usually in acidic electrolytes for the deposition of tin alloys can be added.
  • the use of suitable compounds for the stabilization of the electrolyte is an important requirement for fast and high quality Deposition of bronzes.
  • the electrolyte as Stabilizers and / or complexing agents added gluconates. This is in the Process according to the invention, the preferred use of sodium gluconate as particularly advantageous.
  • the concentration of stabilizers and / or Complexing agent is 0 to 50 g / l electrolyte, preferably 20 to 30 g / l electrolyte.
  • the antioxidant compounds are preferred from the class of Dihydroxybenzenes for example mono- or polyhydroxyphenyl such Catechol or phenolsulfonic acid used.
  • the concentration of Antioxidant is 0 to 5 g / l electrolyte.
  • the Electrolyte Hydroquinone as antioxidant.
  • the implementation of the method according to the invention enables the deposition of bronzes on different substrates.
  • everyone can conventional materials are used for the production of electronic components.
  • inventive method in particular hard and Wear-resistant bronze coatings on materials such as plain bearings etc. deposited.
  • the method according to the invention is advantageously used, which is particularly advantageous in these areas, the deposition of Multi-alloy containing tin, copper, zinc and bismuth, affects.
  • a very particular advantage is that with the method according to the invention so-called "real" bronzes can be deposited, which have a copper content > 60%, the copper content depending on the desired property up to May be 95 wt .-%.
  • the ratio of copper content to Tin content in the electrolyte has a significant influence on the properties Hardness and color of bronze coatings. So be at a ratio Tin / copper of 40/60 silver-colored coatings, so-called white bronzes deposited, which are relatively soft. At a tin / copper ratio from 20/80 arise yellow gold colored coatings, so-called yellow bronzes, and at a tin / copper ratio of 10/90 produces red gold-colored coatings, so-called red bronzes.
  • the Electrolytes in addition to a different copper content, in addition to additives such as For example, brighteners added.
  • the electrolyte contains Brighteners from the class of aromatic carbonyl compounds and / or ⁇ , ⁇ -unsaturated carbonyl compounds.
  • the concentration of brighteners is 0 to 5 g / l electrolyte.
  • Electrolyte composition :
  • the base electrolyte of the strongly acidic electrolyte according to the invention essentially comprises (per liter of the electrolyte) 2 - 75 g divalent tin, 2 - 70 g divalent copper, 2 - 40 g an aromatic, nonionic wetting agent and 140 - 382 g a mineral and / or alkylsulfonic acid
  • further constituents can be added to the electrolyte: 0-10 g an anionic and / or aliphatic, nonionic wetting agent, 0 - 50 g a stabilizer and / or complexing agent, 0 - 5 g an antioxidant, 0 - 5 g a shine agent 0 - 5 g trivalent bismuth 0 - 25 g divalent zinc
  • Example 1 red bronze 4 g / l Sn 2+ 18 g / l Cu 2+ 286 g / l methane 3 g / l aromatic, nonionic wetting agent 0.4 g / l aliphatic, nonionic wetting agent 2 g / l Antioxidant 20 mg / l complexing
  • Example 2a (yellow bronze) 4 g / l Sn 2+ 18 g / l Cu 2+ 240 g / l methane 32.2 g / l aromatic, nonionic wetting agent 2 g / l Antioxidant 25 g / l Stabilizer / complexing agent
  • Example 2b (yellow bronze) 4 g / l Sn 2+ 18 g
  • Example 5 (high ductility) 4 g / l Sn 2+ 18 g / l Cu 2+ 238 g / l methane 32.2 g / l aromatic, nonionic wetting agent 3 mg / l brightener 2 g / l Antioxidant 25 g / l Stabilizer / complexing agent 20 g / l ZnSO 4
  • Example 6 (Hardness) 4 g / l Sn 2+ 18 g / l Cu 2+ 238 g / l methane 32.2 g / l aromatic, nonionic wetting agent 2 g / l Antioxidant 25 g / l Stabilizer / complexing agent 0.1 g / l Bi 3+
  • Example 7 (yellow bronze) 14.5 g / l Sn 2+ 65.5 g / l Cu 2+ 382 g / l methane 32.2 g / l aromatic, nonionic wetting agent
  • Example no Coating / Proportions in% by weight Properties of the coating sn Cu Zn Bi hardness ductility shine colour 1 10 90 - - 180 HV 50 ++ Yes red 2a 20 80 - - 283 HV 50 ⁇ Yes yellow 2 B 20 80 - - 317 HV 50 ⁇ Yes yellow 3 40 60 - - 360 HV 50 ⁇ Yes White 4 90 10 - - - - No White 5 20 80 ⁇ 1 - - +++ Yes yellow 6 20 80 - ⁇ 1 345 HV 50 - Yes yellow 7 20 80 ⁇ 1 - - ++ Yes yellow

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electroplating And Plating Baths Therefor (AREA)
  • Electroplating Methods And Accessories (AREA)
  • Chemically Coating (AREA)
EP02022718.7A 2002-10-11 2002-10-11 Methode et électrolyte pour la deposition galvanique des bronzes Revoked EP1408141B1 (fr)

Priority Applications (7)

Application Number Priority Date Filing Date Title
ES02022718T ES2531163T3 (es) 2002-10-11 2002-10-11 Procedimiento y electrolito para la deposición galvánica de bronces
EP02022718.7A EP1408141B1 (fr) 2002-10-11 2002-10-11 Methode et électrolyte pour la deposition galvanique des bronzes
CN2003801012538A CN1703540B (zh) 2002-10-11 2003-10-10 电沉积青铜的方法
PCT/EP2003/011229 WO2004035875A2 (fr) 2002-10-11 2003-10-10 Procede de depot galvanique de bronzes
KR1020057004846A KR100684818B1 (ko) 2002-10-11 2003-10-10 청동의 전해석출 방법
JP2004544134A JP4675626B2 (ja) 2002-10-11 2003-10-10 ブロンズ電析法及び電解質
US10/531,142 US20060137991A1 (en) 2002-10-11 2003-10-10 Method for bronze galvanic coating

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP02022718.7A EP1408141B1 (fr) 2002-10-11 2002-10-11 Methode et électrolyte pour la deposition galvanique des bronzes

Publications (2)

Publication Number Publication Date
EP1408141A1 true EP1408141A1 (fr) 2004-04-14
EP1408141B1 EP1408141B1 (fr) 2014-12-17

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ID=32010957

Family Applications (1)

Application Number Title Priority Date Filing Date
EP02022718.7A Revoked EP1408141B1 (fr) 2002-10-11 2002-10-11 Methode et électrolyte pour la deposition galvanique des bronzes

Country Status (7)

Country Link
US (1) US20060137991A1 (fr)
EP (1) EP1408141B1 (fr)
JP (1) JP4675626B2 (fr)
KR (1) KR100684818B1 (fr)
CN (1) CN1703540B (fr)
ES (1) ES2531163T3 (fr)
WO (1) WO2004035875A2 (fr)

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1630258A1 (fr) * 2004-08-28 2006-03-01 Enthone, Inc. Procédé pour la déposition électrolytique de cuivre
EP1803837A1 (fr) 2005-11-25 2007-07-04 Enthone, Inc. Procédé et appareillage pour le nettoyage de solutions de traitement
WO2007134843A2 (fr) * 2006-05-24 2007-11-29 Atotech Deutschland Gmbh Composition de placage métallique et procédé de dépôt de cuivre-zinc-étain appropriés pour fabriquer une photo-pile à film mince
EP1874982A1 (fr) * 2005-04-14 2008-01-09 Enthone, Inc. Methode d'electrodeposition de bronzes
CN100368924C (zh) * 2005-05-31 2008-02-13 西北工业大学 一种非周期性红外波段负磁导率材料
EP1961840A1 (fr) * 2007-02-14 2008-08-27 Umicore Galvanotechnik GmbH Electrolyte de cuivre-étain et procédé pour le dépôt de couches de bronze
EP2116634A1 (fr) 2008-05-08 2009-11-11 Umicore Galvanotechnik GmbH Electrolyte de cuivre-zinc modifié et procédé de déposition de couches de bronze
DE102008032398A1 (de) 2008-07-10 2010-01-14 Umicore Galvanotechnik Gmbh Verbesserter Kupfer-Zinn-Elektrolyt und Verfahren zur Abscheidung von Bronzeschichten
DE102011008836A1 (de) 2010-08-17 2012-02-23 Umicore Galvanotechnik Gmbh Elektrolyt und Verfahren zur Abscheidung von Kupfer-Zinn-Legierungsschichten
EP2565297A3 (fr) * 2011-08-30 2013-04-24 Rohm and Haas Electronic Materials LLC Promotion de l'adhérence de bronze blanc exempt de cyanure

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Publication number Priority date Publication date Assignee Title
US7296370B2 (en) * 2004-09-24 2007-11-20 Jarden Zinc Products, Inc. Electroplated metals with silvery-white appearance and method of making
WO2006036479A1 (fr) * 2004-09-24 2006-04-06 Jarden Zinc Products, Inc. Metaux deposes par electrodeposition presentant un aspect blanc argente et procede de production
JP5642928B2 (ja) 2007-12-12 2014-12-17 ローム・アンド・ハース・エレクトロニック・マテリアルズ，エル．エル．シー． 青銅の電気めっき
US8426241B2 (en) 2010-09-09 2013-04-23 International Business Machines Corporation Structure and method of fabricating a CZTS photovoltaic device by electrodeposition
CN102605394B (zh) * 2012-03-07 2015-02-18 深圳市华傲创表面技术有限公司 一种无氰酸性白铜锡电镀液
JP6101510B2 (ja) * 2013-02-18 2017-03-22 株式会社シミズ 非シアン銅−錫合金めっき浴
CN106661752B (zh) * 2014-08-08 2021-08-10 奥野制药工业株式会社 铜－锡合金镀敷浴
US11597637B2 (en) 2018-02-22 2023-03-07 Vis, Llc Under hoist support stand
EP3540097A1 (fr) 2018-03-13 2019-09-18 COVENTYA S.p.A. Produits galvanisés et bain électrolytique approprié pour fournir de tels produits
US10906789B2 (en) * 2018-09-05 2021-02-02 Vis, Llc Power unit for a floor jack

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EP1001054A2 (fr) * 1998-11-05 2000-05-17 C. Uyemura & Co, Ltd Bain pour le dépôt électrolytique d'un alliage étain-cuivre et procédé de déposition utilisant ce bain
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EP1091023A2 (fr) * 1999-10-08 2001-04-11 Shipley Company LLC Composition d'alliage et procédé de plaquage
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EP1091023A2 (fr) * 1999-10-08 2001-04-11 Shipley Company LLC Composition d'alliage et procédé de plaquage
EP1111097A2 (fr) * 1999-12-22 2001-06-27 Nippon MacDermid Co., Ltd. Solution de dépôt électrolytique d'une alliage étain-cuivre brilliante
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Cited By (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1630258A1 (fr) * 2004-08-28 2006-03-01 Enthone, Inc. Procédé pour la déposition électrolytique de cuivre
EP1874982A1 (fr) * 2005-04-14 2008-01-09 Enthone, Inc. Methode d'electrodeposition de bronzes
EP1874982A4 (fr) * 2005-04-14 2011-07-27 Enthone Methode d'electrodeposition de bronzes
CN100368924C (zh) * 2005-05-31 2008-02-13 西北工业大学 一种非周期性红外波段负磁导率材料
EP1803837A1 (fr) 2005-11-25 2007-07-04 Enthone, Inc. Procédé et appareillage pour le nettoyage de solutions de traitement
EP2336394A3 (fr) * 2006-05-24 2011-11-30 ATOTECH Deutschland GmbH Composition de placage métallique et procédé pour le dépôt de cuivre-zinc-étain adapté à la fabrication de cellule solaire à couche mince
WO2007134843A2 (fr) * 2006-05-24 2007-11-29 Atotech Deutschland Gmbh Composition de placage métallique et procédé de dépôt de cuivre-zinc-étain appropriés pour fabriquer une photo-pile à film mince
WO2007134843A3 (fr) * 2006-05-24 2008-11-27 Atotech Deutschland Gmbh Composition de placage métallique et procédé de dépôt de cuivre-zinc-étain appropriés pour fabriquer une photo-pile à film mince
EP2037006A3 (fr) * 2006-05-24 2009-08-05 Atotech Deutschland Gmbh Composition de placage métallique et procédé pour le dépôt de cuivre-zinc-étain adapté à la fabrication de cellule solaire à couche mince
EP1961840A1 (fr) * 2007-02-14 2008-08-27 Umicore Galvanotechnik GmbH Electrolyte de cuivre-étain et procédé pour le dépôt de couches de bronze
US8211285B2 (en) 2007-02-14 2012-07-03 Umicore Galvanotechnik Gmbh Copper-tin electrolyte and method for depositing bronze layers
EP2116634A1 (fr) 2008-05-08 2009-11-11 Umicore Galvanotechnik GmbH Electrolyte de cuivre-zinc modifié et procédé de déposition de couches de bronze
DE102008032398A1 (de) 2008-07-10 2010-01-14 Umicore Galvanotechnik Gmbh Verbesserter Kupfer-Zinn-Elektrolyt und Verfahren zur Abscheidung von Bronzeschichten
DE102011008836A1 (de) 2010-08-17 2012-02-23 Umicore Galvanotechnik Gmbh Elektrolyt und Verfahren zur Abscheidung von Kupfer-Zinn-Legierungsschichten
WO2012022689A1 (fr) 2010-08-17 2012-02-23 Umicore Galvanotechnik Gmbh Electrolyte et procédé de dépôt de couches en alliage de cuivre-étain
DE102011008836B4 (de) * 2010-08-17 2013-01-10 Umicore Galvanotechnik Gmbh Elektrolyt und Verfahren zur Abscheidung von Kupfer-Zinn-Legierungsschichten
EP2565297A3 (fr) * 2011-08-30 2013-04-24 Rohm and Haas Electronic Materials LLC Promotion de l'adhérence de bronze blanc exempt de cyanure
EP2660360A1 (fr) * 2011-08-30 2013-11-06 Rohm and Haas Electronic Materials LLC Promotion de l'adhérence de bronze blanc exempt de cyanure

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Publication number Publication date
CN1703540A (zh) 2005-11-30
JP2005537394A (ja) 2005-12-08
US20060137991A1 (en) 2006-06-29
KR100684818B1 (ko) 2007-02-22
KR20050059174A (ko) 2005-06-17
JP4675626B2 (ja) 2011-04-27
WO2004035875A3 (fr) 2005-04-14
WO2004035875A2 (fr) 2004-04-29
CN1703540B (zh) 2010-10-06
ES2531163T3 (es) 2015-03-11
EP1408141B1 (fr) 2014-12-17

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